Activation processes for monolith adsorbents

Abstract

An improved method for preparing and activating monolith adsorbents is disclosed. A regeneration gas is passed through the formed monolith adsorbent at a temperature sufficient to decompose at least part of the binding agents in the adsorbent. The present invention also provides for the use of the treated adsorbent monoliths in separating gases in cyclical separation processes such as vacuum swing adsorption processes.

Having thus described the invention, what we claim is:  
     
       1. A process for removing binding agents from a monolith structure while activating the adsorbent in said monolith structure, comprising passing a regeneration gas through said monolith at a temperature which will decompose the binding agents in said monolith. 
     
     
       2. The process as claimed in  claim 1  wherein said monolith structure contains one or more adsorbent materials. 
     
     
       3. The process as claimed in  claim 1  wherein said regeneration gas is selected from the group consisting of nitrogen, argon, hydrogen, oxygen, nitrous oxide, ozone, and mixtures thereof. 
     
     
       4. The process as claimed in  claim 1  wherein said temperature is sufficient to remove greater than 50% of the binding agents. 
     
     
       5. The process as claimed in  claim 1  wherein said temperature is sufficient to remove between 70% and 98% of the binding agents. 
     
     
       6. The process as claimed in  claim 1  wherein said temperature is in a range of about 300° C. to about 500° C. 
     
     
       7. The process as claimed in  claim 1  wherein said binding agents are selected from the group consisting of acrylic latex, starch, polyvinyl alcohols, acrylics, polyurethane, polyethylene glycol, polypropylene glycol, polyacrylic acid, polyamide and polyamine. 
     
     
       8. The process as claimed in  claim 2  wherein said adsorbent materials are selected from the group consisting of zeolite type X, zeolite type A, ZSM-3, EMT, EMC-2, ZSM-18, ZK-5, ZSM-5, ZSM-11, β, L, chabazite, offretite, erionite, mordenite, gmelinite, mazzite, and mixtures thereof, alumina, CMS, silica, silica gel, amorphous aluminosilicate and a clay materials. 
     
     
       9. The process as claimed in  claim 7  wherein said adsorbent material comprises a zeolite type X or zeolite type A containing lithium, lithium and bivalent cations, or lithium and trivalent cations. 
     
     
       10. The process as claimed in  claim 9  wherein said zeolite is X with an Si/Al ratio less than 1.08. 
     
     
       11. The process as claimed in  claim 7  wherein said zeolites are sodium-containing zeolites. 
     
     
       12. The process as claimed in  claim 7  wherein said adsorbent material is selected from the group consisting of type X zeolite, type A zeolite, and mordenite. 
     
     
       13. The process as claimed in  claim 10  wherein said zeolites are low silicon type X zeolites with Si/Al ratio of 0.9 to 1.25. 
     
     
       14. The process as claimed in  claim 12  wherein said zeolites are low silicon type X zeolites with Si/Al ratio of 1.0 to 1.1. 
     
     
       15. The process as claimed in  claim 14  wherein said zeolite is X with an Si/Al ratio less than 1.08. 
     
     
       16. The process as claimed in  claim 9  wherein said adsorbent material is selected from the group consisting of alumina and CMS. 
     
     
       17. An improved process for preparing a monolith adsorbent comprising the steps of: forming a slurry comprising water, fiber, binding agents, adsorbent and flocculating agent; forming paper from said slurry; forming a monolith containing said paper; the improvement comprising passing a regeneration gas stream through said monolith at a temperature sufficient to decompose at least part of the binding agent present in said adsorbent. 
     
     
       18. The process as claimed in  claim 17  wherein said monolith structure contains one or more adsorbent materials. 
     
     
       19. The process as claimed in  claim 17  wherein said regeneration gas is selected from the group consisting of nitrogen, argon, hydrogen, oxygen, nitrous oxide, ozone, and mixtures thereof. 
     
     
       20. The process as claimed in  claim 17  wherein said temperature is sufficient to remove greater than 50% of the binding agents. 
     
     
       21. The process as claimed in  claim 17  wherein said temperature is sufficient to remove between 70% and 98% of the binding agents. 
     
     
       22. The process as claimed in  claim 21  wherein said temperature is in a range of about 300° C. to about 500° C. 
     
     
       23. The process as claimed in  claim 17  wherein said binding agents are selected from the group consisting of acrylic latex, starch, polyvinyl alcohols, acrylics, polyurethane, polyethylene glycol, polypropylene glycol, polyacrylic acid, polyamide and polyamine. 
     
     
       24. The process as claimed in  claim 18  wherein said adsorbent materials are selected from the group consisting of zeolite type X, zeolite type A, ZSM-3, EMT, EMC-2, ZSM-18, ZK-5, ZSM-5, ZSM-11, β, L, chabazite, offretite, erionite, mordenite, gmelinite, mazzite, and mixtures thereof, alumina, CMS, silica, silica gel, amorphous aluminosilicate and a clay materials. 
     
     
       25. The process as claimed in  claim 17  wherein said adsorbent material is a zeolite type X or zeolite type A containing lithium, lithium and bivalent cations, or lithium and trivalent cations. 
     
     
       26. The process as claimed in  claim 25  wherein said zeolite is X with an Si/Al ratio less than 1.08. 
     
     
       27. The process as claimed in  claim 24  wherein said zeolites are sodium-containing zeolites. 
     
     
       28. The process as claimed in  claim 24  wherein said adsorbent material is selected from the group consisting of type X zeolite, type A zeolite, and mordenite. 
     
     
       29. The process as claimed in  claim 28  wherein said zeolites are low silicon type X zeolites with Si/Al ratio of 0.9 to 1.25. 
     
     
       30. The process as claimed in  claim 29  wherein said zeolites are low silicon type X zeolites with Si/Al ratio of 1.0 to 1.1. 
     
     
       31. The process as claimed in  claim 30  wherein said zeolite is X with an Si/Al ratio less than 1.08. 
     
     
       32. The process as claimed in  claim 24  wherein said adsorbent material is selected from the group consisting of alumina and CMS. 
     
     
       33. A method of separating a first gaseous component from a gas mixture comprising a first gaseous component and a second gaseous component comprising: 
       (a) passing the gaseous mixture into an adsorption zone containing a monolith adsorbent through which an regeneration gas has been passed at a temperature which will decompose at least part of the binding agents in said monolith adsorbent and wherein said monolith adsorbent is capable of separating said first gaseous component from said second gaseous component; and  
       (b) recovering the non-preferentially adsorbed gaseous component from said adsorption zone.  
     
     
       34. The method as claimed in  claim 33  wherein said gaseous mixture is air and said first and said second gaseous components are oxygen and nitrogen. 
     
     
       35. The process as claimed in  claim 33  wherein said monolith structure contains one or more adsorbent materials. 
     
     
       36. The process as claimed in  claim 33  wherein said regeneration gas is selected from the group consisting of nitrogen, argon, hydrogen, oxygen, nitrous oxide, ozone, and mixtures thereof. 
     
     
       37. The process as claimed in  claim 33  wherein said temperature is sufficient to activate the adsorbent materials in said monolith. 
     
     
       38. The process as claimed in  claim 33  wherein said temperature is sufficient to remove greater than 50% of the binding agents. 
     
     
       39. The process as claimed in  claim 33  wherein said temperature is sufficient to remove between 70% and 98% of the binding agents. 
     
     
       40. The process as claimed in  claim 33  wherein said temperature is in a range of about 300° C. to about 500° C. 
     
     
       41. The process as claimed in  claim 33  wherein said binding agents are selected from the group consisting of acrylic latex, starch, polyvinyl alcohols, acrylics, polyurethane, polyethylene glycol, polypropylene glycol, polyacrylic acid, polyamide and polyamine. 
     
     
       42. The process as claimed in  claim 33  wherein said adsorbent materials are selected from the group consisting of zeolite type X, zeolite type A, ZSM-3, EMT, EMC-2, ZSM-18, ZK-5, ZSM-5, ZSM-11, β, L, chabazite, offretite, erionite, mordenite, gmelinite, mazzite, and mixtures thereof, alumina, CMS, silica, silica gel, amorphous aluminosilicate and a clay materials. 
     
     
       43. The process as claimed in  claim 42  wherein said adsorbent material is a zeolite type X or zeolite type A containing lithium, lithium and bivalent cations, or lithium and trivalent cations. 
     
     
       44. The process as claimed in  claim 43  wherein said zeolite is X with an Si/Al ratio less than 1.08. 
     
     
       45. The process as claimed in  claim 43  wherein said zeolites are sodium-containing zeolites. 
     
     
       46. The process as claimed in  claim 45  wherein said adsorbent material is selected from the group consisting of type X zeolite, type A zeolite, and mordenite. 
     
     
       47. The process as claimed in  claim 46  wherein said zeolites are low silicon type X zeolites with Si/Al ratio of 0.9 to 1.25. 
     
     
       48. The process as claimed in  claim 47  wherein said zeolites are low silicon type X zeolites with Si/Al ratio of 1.0 to 1.1. 
     
     
       49. The process as claimed in  claim 48  wherein said zeolite is X with an Si/Al ratio less than 1.08. 
     
     
       50. The process as claimed in  claim 42  wherein said adsorbent material is selected from the group consisting of alumina and CMS.